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中国科学院大学学报 ›› 2009, Vol. 26 ›› Issue (3): 310-318.DOI: 10.7523/j.issn.2095-6134.2009.3.004

• 论文 • 上一篇    下一篇

氟化磷酸铟的合成与表征

李兴亮1,2, 苏哲2, 李首建2   

  1. 1. 中国工程物理研究院核物理与化学研究所, 绵阳 621900;
    2. 四川大学化学学院, 成都 610064
  • 收稿日期:2008-10-07 修回日期:2008-12-22 发布日期:2009-05-15
  • 通讯作者: 李兴亮
  • 基金资助:

    supported by National Natural Science Foundation of China (20571053) 

Synthesis and characterization of fluorinated indium phosphate

LI Xing-Liang1,2, SU Zhe2, LI Shou-Jian2   

  1. 1. Institute of Nuclear Physics and Chemistry, Chinese Academy of Engineering Physics, Mianyang 621900, China;
    2. College of Chemistry, Sichuan University, Chengdu 610064, China
  • Received:2008-10-07 Revised:2008-12-22 Published:2009-05-15
  • Supported by:

    supported by National Natural Science Foundation of China (20571053) 

摘要:

以尿素与氯化胆碱的低共熔点液体同时兼做溶剂和模板传递剂,在离子热体系下合成了InF2 2(NH4)3.采用同样的低共熔点液体在水热条件下不能得到相同的产物.产物晶体参数如下:C2/c(No.15)空间群,a=13.799(3) ,b=5.091(2) ,c=16.094(3) , β=112.942(16)°,V=1041.2(5) 3 and Z=4; R1=0.0582,wR2=0.1589. 在产物结构中,In八面体与P四面体形成四员环,顶角相连形成链状结构.客体铵分子填充于链与链间的空穴中,通过氢键与骨架中的F原子,P—OH和 P O 基团作用,链与链间靠范德华力吸引进而形成层状结构.产物进一步通过粉末XR, EDX, IR, XPS和TG/DTA进行表征.

关键词: 低共熔点液体, 离子热合成, 氟化磷酸铟

Abstract:

A fluorinated indiumphosphate, InF2 2(NH4)3, has been prepared under ionothermal condition using deep-eutectic solvents of choline chloride and urea as solvent and template-delivery agents. The same material can not be observed with the presence of the same deep-eutectic mixture under normal hydrothermal process. The compound crystallized in the monoclinic system, space group C2/c (No.15) with cell parameters a=13.799(3) , b=5.091(2) , c=16.094(3) , β=112.942(16)°, V=1041.2(5) 3 and Z=4; the final residual factors were R1=0.0582 and wR 2=0.1589. The structure is built from an infinite chain composed of interconnected 4-member ring with formula of InF2 3-2. The guest ammonium are hydrogen bonded to the F atoms located in two outmost vertexes of indium octahedral and terminal P—OH and P O groups in the chain respectively. The integrated framework is formed by van der Waals forces holding the chains together as extensive H bond array exists in the compound. The further characterizations of the compound have been performed by X-ray powder diffraction, EDX, IR, XPS and TG/DTA analyses.

Key words: deep-eutectic solvents, ionothermal synthesis, fluorinated indiumphosphate

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